PAH Residues in Honey by Ultrasound-Vortex-Assisted Liquid-Liquid Micro-Extraction Followed by GC-FID/IT-MS

Abstract

Polycyclic aromatic hydrocarbon (PAH) residue concentrations have been measured in honey samples collected on the Italian market. An ultrasound-vortex-assisted dispersive liquid-liquid micro-extraction (UVALLME) procedure coupled with a gas chromatography flame ionization detector or ion trap mass spectrometry (GC-IT/MS) is proposed for fast analysis of fluorene, phenanthrene, anthracene, fluoranthene, pyrene, chrysene, benzo(b)fluoranthene, benzo(a)pyrene, and benzoperylene. Different analytical parameters such as extraction solvent and relative volume, best extraction time, pH, NaCl concentration, and reproducibility at low and high concentrations were optimized. Under optimal conditions, the recoveries range from 95 to 107% and correlation coefficients range from 0.893 to 0.995 whereas the limits of detection (LODs) and limits of quantification (LOQs) are ≥36 and ≥41 ng g−1 in GC-FID and 0.030 and 0.069 ng g−1 in GC-IT/MS, respectively. The precision, expressed as relative standard deviations (RSDs), is ≤7.4 and ≤5.2% for low and high PAH concentration levels, respectively. The whole proposed methodology, demonstrated to be simple, reproducible, and sensible, has been applied to the determination of trace PAHs in five honey samples.